US3653979A - Process for the production of a steel exhibiting consistently low weight loss test values - Google Patents
Process for the production of a steel exhibiting consistently low weight loss test values Download PDFInfo
- Publication number
- US3653979A US3653979A US841551A US3653979DA US3653979A US 3653979 A US3653979 A US 3653979A US 841551 A US841551 A US 841551A US 3653979D A US3653979D A US 3653979DA US 3653979 A US3653979 A US 3653979A
- Authority
- US
- United States
- Prior art keywords
- steel
- weight loss
- loss test
- sulfide
- low weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 16
- 229910000831 Steel Inorganic materials 0.000 title abstract description 36
- 239000010959 steel Substances 0.000 title abstract description 36
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 230000004580 weight loss Effects 0.000 title description 12
- 230000001747 exhibiting effect Effects 0.000 title description 3
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052977 alkali metal sulfide Inorganic materials 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052717 sulfur Inorganic materials 0.000 abstract description 9
- 239000011593 sulfur Substances 0.000 abstract description 9
- 238000009792 diffusion process Methods 0.000 abstract description 5
- 235000014171 carbonated beverage Nutrition 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000002344 surface layer Substances 0.000 abstract description 4
- 238000005097 cold rolling Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 13
- -1 sulfide ions Chemical class 0.000 description 7
- 230000001681 protective effect Effects 0.000 description 6
- 239000005028 tinplate Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 238000009628 steelmaking Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 235000008730 Ficus carica Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- POWFTOSLLWLEBN-UHFFFAOYSA-N tetrasodium;silicate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])[O-] POWFTOSLLWLEBN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/62—Treatment of iron or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
Definitions
- the strip Following the cold reduction of the steel strip to the required gauge the strip must be cleaned to remove the residual oils remaining on the strip after rolling. This can be achieved by immersion in or spraying of the conventional hot alkaline cleaning solutions based on such materials as sodium hydroxide, sodium carbonate and sodium orthosilicate. The strip should be thoroughly rinsed with water before passing on to the sulfiding step.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Chemical Treatment Of Metals (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Steel strip to be used in the manufacture of carbonated beverage packs is treated to incorporate sulfur into its surface layers by diffusion during the annealing cycle that is normally conducted after cold rolling and cleaning operations. The steel is first treated with an aqueous sulfide solution, dried and then heated in a conventional annealing furnace.
Description
United States Patent Whitton et al.
[451 Apr. 4, 1972 [54] PROCESS FOR THE PRODUCTION OF A STEEL EXHIBITING CONSISTENTLY LOW WEIGHT LOSS TEST VALUES [72] Inventors: Richard Wilfred Whitton, Figtree, New South Wales; Ronald Herbert Southall; Michael William McKenzie, both of Keiraville, New South Wales; Ralph Edward Shackleford, West Wollongong, New South Wales, all of Australia [73] Assignee: Australian Iron & Steel Pty. Limited, Sydney, New South Wales, Australia [22] Filed: July 14, 1969 [21] Appl. No.: 841,551
[30] Foreign Application Priority Data July 25, 1968 Australia ..4l21l/68 [52] US. Cl ..l48/6.24, 148/14 2,844,497 7/1958 Henricks l 48/6.24
Primary ExaminerRalph S. Kendall Attorney-Wenderoth, Lind and Ponack [57] ABSTRACT Steel strip to be used in the manufacture of carbonated beverage packs is treated to incorporate sulfur into its surface layers by diffusion during the annealing cycle that is normally conducted after cold rolling and cleaning operations. The steel is first treated with an aqueous sulfide solution, dried and then heated in a conventional annealing furnace.
4 Claims, No Drawings PROCESS FOR THE PRODUCTION OF A STEEL EXHIBITING CONSISTENTLY LOW WEIGHT LOSS TEST VALUES This invention relates to a process for treating steel to give a superior performance in the Weight Loss Test. More particularly this process is especially applicable to steel strip that is electro tin plated and used in the manufacture of carbonated beverage packs.
A Weight Loss Test has been developed to provide an accelerated corrosion test that will assess the performance of steels used in the manufacture of electrolytic tin plate particularly where the contemplated end use is in the manufacture of containers for application in the carbonated beverage packaging field. The essential features of the Weight Loss Test are as follows:
A preweighed sample of steel or detinned and de-alloyed tin plate, 4 square centimetres in area, is immersed in a deaerated test solution of synthetic Cola medium for 96 hours. During the test the reaction vessel and solution is kept deaerated by continuous flushing with carbon dioxide. After the immersion the weight loss is determined, and for convenience the weight loss is converted to micro amps cm. The lower the value obtained the better the tin plate.
Increases in the concentration of sulfur in the steel, as determined by analysis during steelmaking in the Open Hearth furnace, is known to influence the Weight Loss Test values. However it is difficult to control the sulfur content within narrow limits to guarantee specific properties during steelmaking practice. Moreover a general increase in the sulfur content of the steel is undesirable and may give rise to difficulties in the rolling of the steel ingots into steel strip. Furthermore sulfur introduced during steelmaking is prone to segregation and thus will be depicted in the area adjacent to the steel strip surface where its effects are required.
The object of this invention is to provide a process which will produce steel strip that will exhibit consistently low Weight Loss Test values.
Another object of this invention is that the steel strip can be modified without seriously disrupting the major processing steps in the production of electrolytic tin plate from the steelmaking through to the final plating operations.
These objects are achieved by incorporating sulfur into the surface layers of the steel by diffusion during the annealing cycle that is conducted after cold rolling and cleaning operations. The process involves contacting the steel strip with an aqueous solution of sulfide ions, driving off the water from the surface film and annealing the coated steel strip in a neutral or reducing atmosphere.
Following the cold reduction of the steel strip to the required gauge the strip must be cleaned to remove the residual oils remaining on the strip after rolling. This can be achieved by immersion in or spraying of the conventional hot alkaline cleaning solutions based on such materials as sodium hydroxide, sodium carbonate and sodium orthosilicate. The strip should be thoroughly rinsed with water before passing on to the sulfiding step. t
A film containing sulfide is formed on the surface of the steel strip by exposing the cleaned steel strip to an aqueous solution of sulfide ions. The sulfide containing solution may be applied with sprays or by strip immersion in the solution. However it is essential that the space surrounding the application apparatus be adequately ventilated to remove hydrogen sulfide.
The sulfide-containing solution consists of an aqueous solution of sulfide ions in the concentration range 0.15 to 1.5 percent W/W and at a pH of between 7.0 to 9.5. The sulfide ions may be supplied by dissolving in water any of the alkalimetal sulfides to give the required concentration of sulfide ions. The preferred method of preparing the solution is to dissolve sodium sulfide in water to give a solution containing 0.4 percent W/W sulfide ions and then adjust the pH by the addition of sulfuric acid until a piece of clean cold rolled steel, when immersed in the solution, blackens. The H obtained in this way will normally be m the range pH 8 to The solution temperature is maintained in the range 18 to 35 C. for the purposes of the treatment.
The time of contact between the sulfide-containing solution and the steel strip will depend on the particular solution conditions and the degree of effect required, however, in the preferred method treatment times of between 0.5 and 5.0 seconds are used.
Rinsing the strip with water after the sulfide treatment is not essential but is desirable, particularly when solutions of high sulfide concentrations are used.
The strip should then be dried using any of the conventional techniques such as blasting the steel surface with hot air.
To provide a sulfur enriched steel surface the strip is heat treated in a protective atmosphere to effect the diffusion of the sulfur from the surface film into the surface layers of the steel strip. This may be accomplished in the conventional continuous annealing furnaces or in the conventional batch annealing furnaces.
In the batch annealing furnace the coiled steel strip would be heated to between 600 and 800 C. and held for between 0.5 and 12 hours. A neutral or reducing protective atmosphere is maintained around the coiled steel strip throughout the heat treatment to prevent oxidation. The protective atmosphere may be any of those known to the art. An example is ANX gas containing 5% V/V hydrogen, 95% V/V nitrogen and moisture to give a dewpoint below 40 F.
In the continuous annealing furnace the strip is passed into a furnace zone filled with a neutral or reducing protective atmosphere, known to the art, and held at temperatures in the range 600 to 800 C. for between 20 seconds and seconds. The strip is then cooled in the presence of the protective atmosphere.
The steel strip so prepared can then be processed by the conventional techniques to make electrolytic tin plate that will exhibit low Weight Loss Test values.
What we claim is:
l. A process of preparing a steel strip that will exhibit consistently low Weight Loss Test values, which comprises treating a cold rolled, clean steel strip with an aqueous solution containing sulphide ions derived from a sulfide selected from the group consisting of alkali metal sulfides in a concentration in the range of from 0.15 to 1.5 percent W/W and at a pH of between 7 .0 and 9.5 to form a sulfide film on the strip, and then, after drying, heat-treating the steel strip in a neutral or reducing protective atmosphere at a temperature of between 600 and 800 C. sufficiently to cause diffusion of the sulfide film into the surface of the steel strip.
2. A process as claimed in claim 1, wherein the heat treatment is carried out for between 20 and 90 seconds in a continuous annealing furnace.
3. A process as claimed in claim 1, wherein the heat treatment is carried out for between 0.5 and 12 hours in a conventional batch annealing furnace.
4. A process according to claim 1, wherein the alkali metal sulfide is sodium sulfide.
Claims (3)
- 2. A process as claimed in claim 1, wherein the heat treatment is carried out for between 20 and 90 seconds in a continuous annealing furnace.
- 3. A process as claimed in claim 1, wherein the heat treatment is carried out for between 0.5 and 12 hours in a conventional batch annealing furnace.
- 4. A process according to claim 1, wherein the alkali metal sulfide is sodium sulfide.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU41211/68A AU424391B2 (en) | 1968-07-25 | 1968-07-25 | A process forthe production ofa steel exhibiting consistently low weight loss test values |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3653979A true US3653979A (en) | 1972-04-04 |
Family
ID=3728586
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US841551A Expired - Lifetime US3653979A (en) | 1968-07-25 | 1969-07-14 | Process for the production of a steel exhibiting consistently low weight loss test values |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US3653979A (en) |
| JP (1) | JPS4827582B1 (en) |
| AU (1) | AU424391B2 (en) |
| GB (1) | GB1267527A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4042425A (en) * | 1971-10-11 | 1977-08-16 | Kawasaki Steel Corporation | Process of pretreating cold-rolled steel sheet for annealing |
| US4206004A (en) * | 1971-10-11 | 1980-06-03 | Kawasaki Steel Corporation | Process of pretreating cold-rolled steel sheet for annealing |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS516604B1 (en) * | 1971-04-26 | 1976-03-01 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2266380A (en) * | 1940-05-18 | 1941-12-16 | Standard Oil Co California | Pretreatment of metal bearing surfaces |
| US2707159A (en) * | 1947-02-19 | 1955-04-26 | Lubri Case Inc | Wear-resistant ferrous metal articles and their production |
| US2844497A (en) * | 1956-12-07 | 1958-07-22 | Devex Corp | Method of applying sulfide coating on wires for drawing and composition therefor |
-
1968
- 1968-07-25 AU AU41211/68A patent/AU424391B2/en not_active Expired
-
1969
- 1969-07-14 US US841551A patent/US3653979A/en not_active Expired - Lifetime
- 1969-07-15 GB GB35689/69A patent/GB1267527A/en not_active Expired
- 1969-07-25 JP JP44058465A patent/JPS4827582B1/ja active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2266380A (en) * | 1940-05-18 | 1941-12-16 | Standard Oil Co California | Pretreatment of metal bearing surfaces |
| US2707159A (en) * | 1947-02-19 | 1955-04-26 | Lubri Case Inc | Wear-resistant ferrous metal articles and their production |
| US2844497A (en) * | 1956-12-07 | 1958-07-22 | Devex Corp | Method of applying sulfide coating on wires for drawing and composition therefor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4042425A (en) * | 1971-10-11 | 1977-08-16 | Kawasaki Steel Corporation | Process of pretreating cold-rolled steel sheet for annealing |
| US4206004A (en) * | 1971-10-11 | 1980-06-03 | Kawasaki Steel Corporation | Process of pretreating cold-rolled steel sheet for annealing |
Also Published As
| Publication number | Publication date |
|---|---|
| GB1267527A (en) | 1972-03-22 |
| AU424391B2 (en) | 1972-05-22 |
| JPS4827582B1 (en) | 1973-08-23 |
| AU4121168A (en) | 1971-01-14 |
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